US6375729B1 - Machinable glass-ceramics - Google Patents
Machinable glass-ceramics Download PDFInfo
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- US6375729B1 US6375729B1 US09/527,196 US52719600A US6375729B1 US 6375729 B1 US6375729 B1 US 6375729B1 US 52719600 A US52719600 A US 52719600A US 6375729 B1 US6375729 B1 US 6375729B1
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- glass
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- micaceous
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/16—Halogen containing crystalline phase
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/20—Protective coatings for natural or artificial teeth, e.g. sealings, dye coatings or varnish
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/70—Preparations for dentistry comprising inorganic additives
- A61K6/71—Fillers
- A61K6/77—Glass
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/70—Preparations for dentistry comprising inorganic additives
- A61K6/78—Pigments
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
- A61K6/807—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising magnesium oxide
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
- A61K6/816—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising titanium oxide
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
- A61K6/818—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising zirconium oxide
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
- A61K6/822—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising rare earth metal oxides
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
- A61K6/824—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising transition metal oxides
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
- A61K6/833—Glass-ceramic composites
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
- A61K6/836—Glass
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C13/00—Dental prostheses; Making same
- A61C13/08—Artificial teeth; Making same
- A61C13/083—Porcelain or ceramic teeth
Definitions
- This invention relates generally to a glass powder, which is crystallizable and forms a sintered micaceous glass-ceramic in a plurality of shades and more specifically to micaceous glass ceramics, which are machinable into various dental articles by conventional tools.
- This material is especially useful for the fabrication of dental restorations using computer assisted design/computer assisted milling (CAD/CAM) devices.
- CAD/CAM computer assisted design/computer assisted milling
- Micaceous glass-ceramic materials i.e. glass-ceramics comprising a crystalline phase that belongs to the mica family such as tetrasilic fluormicas or fluorophlogopite micas
- CAD/CAM materials for dentistry is limited by the inability to produce the required range of shades and translucency paramount for esthetically sound restorations. This severely inhibits widespread use of micaceous materials as dental restoratives considering that the driving force for all-ceramic restorations is esthetics superior to that of porcelain fused-to-metal (PFM) restorations.
- PFM porcelain fused-to-metal
- Dicor MGC available from Dentsply International Inc., Caulk Division, (located in Milford, DE) is a commercially available micaceous dental ceramic for use in CAD/CAM devices, but it is supplied in only two modifications, Dicor MGC—Light and Dicor MGC—Dark.
- Other limitations of micaceous glass-ceramics include high solubility and low strength in comparison to other dental ceramics.
- ProGlassTM ceramic available from CAD/CAM Ventures LLC, (located in Irving, Tex.), which is a sugary-white mica-containing material exhibiting a flexure strength of about 100 to about 150 MPa and a solubility of about 1 mg/cm 2 (1000 ⁇ m/cm 2 ).
- micaceous glass-ceramics exhibit far superior machinability compared to other CAD/CAM ceramics such as sanidine-based Vita Mark II, available from Vita Zahnfabrik (Germany) and leucite-based Pro-Cad from Ivoclar (Lichtenstein), as set forth in “Mechanical Properties of a New Mica-Based Machinable Glass Ceramic For CAD/CAM Restorations” by J. Y. Thompson et al., The Journal of Prosthetic Dentistry, 1996, Vol. 76, No. 6,619-623 and “Machinable Glass-Ceramics Based on Tetrasilicic Mica” by D. G. Grossman, Journal of Am.Cer.Soc., 1972, Vol. 55, No. 9.
- micaceous glass-ceramics such as ProGlassTM which can be machined by carbide tooling using dry processing which is much more cost-effective.
- micaceous glass-ceramics can be much more translucent than very opaceous sanidine glass-ceramics.
- U.S. Pat. Nos. 4,652,312, 4,431,420 and 5,246,889 are each directed to mica-containing ceramics that are formed from glass compositions and are shaped as glass and converted into micaceous glass-ceramics by conventional volume crystallization techniques. Each process involves melting glass batches, casting the glass melts into molds, and crystallizing the glass into micaceous glass-ceramics. There is no discussion providing how to achieve adequate colors and shades to accurately match the color of a person's tooth or how to control the shading of mica containing glass-ceramics. Any mention of colorants appears to be directed to adding the colorants to the glass batch prior to melting. Such process does not effectively control the color of the resulting glass-ceramic.
- each of the processes appears to effect crystallization by performing bulk or volume crystallization. It is difficult to control the color of the micaceous glass-ceramics when utilizing volume crystallization. None of the prior art is concerned with the need to provide a variety of colors and shades to adequately match the color and shade of a patient's teeth.
- the micaceous glass-ceramics comprising silica, magnesium oxide and fluorine in addition to other components listed below.
- the glass-ceramics are useful in the fabrication of single and multi-unit dental restorations including but not limited to orthodontic appliances, bridges, space maintainers, tooth replacement appliances, splints, crowns, partial crowns, dentures, posts, teeth, jackets, inlays, onlays, facing, veneers, facets, implants, abutments, cylinders, and connectors by machining the glass-ceramic using CAM/CAM devices.
- the micaceous glass-ceramics are provided in a shade and color selected from a plurality of shades and colors to adequately match the colors and shades of teeth found in 95% or more of the human population.
- the batch ingredients of the compositions are melted at a temperature in the range of about 1200° to about 1650° C., for a time in the range of about 0.5 to about 8 hours, thereafter it is quenched, and pulverized into powder. Pigments, opacifiers, fluorescing agents and the like are mixed with the powder.
- the powder is then used to form net-shaped or block-shaped pre-forms or blanks to be used in CAD/CAM devices. Blanks are dry-pressed and sintered using a one- or two-step heating cycle at a temperature in the range of about 600° to about 1200° C.
- the sintering is preferably conducted in a vacuum. Occurring simultaneously with sintering, surface crystallization of the starting glass powder yields the amount of mica phase of at least thirty volume percent (30 vol. %) required for machinability as well as strength.
- the present invention provides glass-ceramic compositions comprising a glassy matrix and one or more micaceous phases (e.g., tetrasilic flourmica, fluorophlogopite mica and the like).
- the glass-ceramics are useful in the fabrication of dental restorations.
- the micaceous glass-ceramic compositions contain inter alia, silica, magnesium oxide and fluorine in the ranges given in Table 1 below.
- the glass-ceramic compositions have a combination of properties including high strength and chemical durability useful for dental restorations.
- the glass-ceramics have good machinability, i.e., the ability to be cut or milled by a cutting tool into a dental restorative shape that accurately depicts the original shape of the tooth to be restored or replaced.
- the micaceous glass-ceramics are provided in a shade and color selected from a plurality of shades and colors to adequately match the colors and shades of teeth found in 95% or more of the human population.
- the shades and colors of the glass-ceramics provide the dental technician with the ability to closely and effectively match the color and shade of the patient's tooth or teeth abutting or adjacent to the tooth or teeth that is/are being restored or replaced.
- the shaded micaceous glass-ceramics are manufactured by admixing pigments and other additives to the starting glass powder.
- the powder is formed into pre-forms or blanks and the blanks are concurrently sintered and crystallized.
- the resulting shaded blanks of various shades and translucency levels are consistent with current all-ceramic or porcelain-fused-to-metal (PFM) dental porcelain systems.
- the pre-forms or blanks may be machined into a dental restoration using a CAD/CAM device.
- the glass compositions within the ranges given in Table 1 are melted at a temperature in the range of about 1200° to about 1650° C. and for a time in the range of about 0.5 to about 8 hours, thereafter quenched, and pulverized into powder.
- This powder is sieved to obtain the required particle size and mixed with conventional additives such as pigments, opacifiers, and fluorescing agents, which will produce various colors, shades and translucency levels after sintering and concurrent crystallization have been performed.
- the powder that contains the additives is then used to form net-shaped or block-shaped pre-forms or blanks to be used in CAD/CAM devices.
- the blanks are dry-pressed and sintered using a one- or two-step heating cycle at a temperature in the range of about 600° to about 1200° C. and for a time in the range of about 0.5 to about 4 hours for each step in the cycle.
- the sintering is preferably conducted in a vacuum atmosphere. Occurring simultaneously with sintering, surface crystallization of the starting glass powder yields an amount of mica phase of at least thirty volume percent (30 vol %) required for machinability as well as strength.
- Copending commonly assigned U.S. application Ser. No. 09/458,919, filed on Dec. 10, 1999, and U.S. Pat. No. 5,968,856 to Schweiger discuss volume crystallization and surface crystallization of lithium disilicate glass-ceramics and are hereby incorporated by reference.
- CAD/CAM blanks In mass-production of CAD/CAM blanks, uniaxial pressing or other forming techniques are utilized, e.g. CIP/HIP route whereby green bodies are formed in a CIP (Cold Isostatic Press) and subsequently sintered under pressure in an HIP (Hot Isostatic Press).
- CIP/HIP route whereby green bodies are formed in a CIP (Cold Isostatic Press) and subsequently sintered under pressure in an HIP (Hot Isostatic Press).
- the powder can be mixed with binder and pelletized or extruded.
- Useful CAD/CAM devices include the CERECTM machine (available from Siemens AG), the PROCAMTM machine (available from CAD CAM Ventures LLC in Irving, Tex.) or copy-milling devices such as the CelayTM machine (available from Mikrona Technologie AG).
- Essential for the present invention is an F content in excess of about 14 mole percent (about 5 weight percent). Besides being a constituent of fluormicas, F facilitates surface crystallization. Other ingredients that favor surface crystallization are B 2 O 3 , P 2 O 5 , BaO and Li 2 O.
- Essential for the present invention is the volume fraction, size and aspect ratio of the mica phase in the resultant sintered glass-ceramic.
- An aspect ratio, i.e., ratio of thickness to length, of the mica plate of ⁇ 2 is preferred.
- At least thirty volume percent (30 vol. %) of mica is required to attain machinability.
- At least thirty volume percent (30 vol. %) of the residual glass phase is required for sinterability. Therefore, the mica content is between about 30 and about 70 volume percent, and preferably between about 40 and about 60 volume percent.
- compositions of the present invention are extremely reactive and will dissolve additives (e.g., pigments and fluorescing agents) during sintering of the CAD/CAM blocks.
- additives e.g., pigments and fluorescing agents
- coarser additives e.g., pigments or fluorescing agents
- these additives have an average particle size of about 4 to about 8 microns.
- the average size of the additives is in the range of about 15 to about 35 microns, and more preferably in the range of about 20 to about 30 microns.
- a coating is preferably applied over the core material manufactured from the micaceous glass-ceramic to provide an aesthetically pleasing surface.
- a suitable coating is a ceramic, glass-ceramic, a glass, a glaze and/ or a composite material. It is advantageous that the coating has a coefficient of thermal expansion slightly less than the thermal expansion of the core material.
- the coating is typically applied by sintering the ceramic, glass-ceramic, glass, glaze a composite material onto the micaceous glass-ceramic core.
- a starting glass composition corresponding to the composition set forth in Table 2 below was batched from conventional raw ingredients and melted at 1400° C. for 4 hours in a coarse-grained alumina crucible. The glass melt was quenched into water. The quenched glass was dried and milled into powder. The powder was screened to ⁇ 200 mesh. Commercial pigments and fluorescing agents (yellow from Cerdec Co. (Washington, Pa.), pink from Engelhard Corp. (Iselin, N.J.) and jet black from Standard Ceramic Supply Co. (Carnegie, Pa.)) were added to and blended with the powder. The powder was dry-pressed into 18 ⁇ 18 ⁇ 25 mm 3 blocks.
- the blocks were fired in a vacuum of 20 torr using a two-step heating cycle at 10° C./min to 650° C. and held for 2 hours at this temperature and 10° C./min to 1100° C. and held for 4 hours at this temperature.
- the blocks were sectioned into bars for three-point bend strength tests and small squares for solubility measurements according to ISO 9693 solubility testing standards. The measurements are listed in Table 2 below.
- a starting glass composition corresponding to composition set forth in Table 2 below was batched from conventional raw ingredients and melted at 1400° C. for 4 hours in a coarse-grained alumina crucible. The glass melt was quenched into water. The quenched glass was dried and milled into powder. The powder was screened to ⁇ 200 mesh. Commercial pigments and fluorescing agents were used in concentrations given in Table 3 below. Since it is known that all dental shades can be produced by varying combinations of three basic pigments. i.e., yellow, red (or pink) and blue (or gray or black), the glass-ceramic of this example was shaded using both individual yellow, pink and black pigments and their combinations. Yellow pigments from Cerdec (Washington, Pa.), pink pigments from Engelhard Corp.
- Blocks of lightly shaded glass-ceramics of Example 2 were sent to CAD CAM Ventures LLC (Irving, Tex.) and to DentalMatic Technologies Inc. (Sainte-Laurent, Quebec, Canada) to be evaluated for machinability. They were machined into shapes roughly approaching that of a dental coping. The machinability was evaluated as satisfactory.
- Example 2 powder with the addition of pigments Glass powder of example Yellow Pink Jet Black CIE L*a*b* 2 41720 D320 K-60 Light Source: Wt % Wt % Wt % Wt % D65-10° 99.2687 0.7313 L* 53.31 a* ⁇ 2.47 b* 21.33 C* 21.47 h* 96.62 99.6693 0.3307 L* 55.461 a* 2.10 b* 0.22 C* 2.11 h* 6.06 99.995 0.005 L* 54.67 a* ⁇ 0.31 b* 0.08 C* 0.32 h* 164.84 98.6 1.4 99.3 0.7 99.99 0.01 98.933 0.7313 0.3307 0.005 98.59 0.7 0.7 0.01
- the glass-ceramics of the invention have the capability to provide a wide selection of shades and colors for matching the shades and colors of a person's teeth.
- the glass-ceramics are readily machinable and provide high strength and chemical durability to the dental restorations made therefrom.
Abstract
Description
TABLE 1 |
Compositions of the starting glass powder |
Wt % | Wt % | ||||
Oxide | Mole % | Range 1 | Range 2 | ||
SiO2 | 30-65 | 43-72 | 43-72 | ||
Al2O3 | 0-7 | 3-14 | 0-3 | ||
B2O3 | 0-3 | 0-3 | 0-3 | ||
ZnO | 0-3 | 0-3 | 0-3 | ||
CaO | 0-5 | 0-7 | 0-3 | ||
MgO | 15-33 | 10-30 | 10-30 | ||
TiO2 | 0-3 | 0-3 | 0-3 | ||
BaO + SrO | 0-3 | 0-5 | 0-5 | ||
Li2O | 0-3 | 0-3 | 0-3 | ||
K2O | 0-10 | 0-7 | 7-19 | ||
Na2O | 0-7 | 0-3 | 0-3 | ||
CeO2 + La2O3 + | 0-1 | 0-2 | 0-2 | ||
Tb4O7 | |||||
ZrO2 | 0-4 | 0-10 | 0-10 | ||
F | 14-25 | 5-10 | 5-10 | ||
TABLE 2 |
Compositions of glass-ceramics in |
Examples 1 and 2 |
Wt % | Wt % | |||
Oxide | Example 1 | Example 2 | ||
SiO2 | 40.8 | 61.0 | ||
Al2O3 | 11.6 | 0.5 | ||
B2O3 | 0 | 0 | ||
ZnO | 0 | 0 | ||
CaO | 5.5 | 0 | ||
MgO | 27.4 | 17.2 | ||
TiO2 | 0 | 0 | ||
BaO | 0 | 0 | ||
Li2O | 0 | 0 | ||
K2O | 1.5 | 13.1 | ||
Na2O | 0 | 0 | ||
CeO2 | 0 | 0 | ||
ZrO2 | 8.3 | 5 | ||
F | 8.6 | 5.6 | ||
3-Pt bend | 196 ± 24 | >100 | ||
strength | ||||
(MPa) | ||||
ISO 9693 | 8 | <100 | ||
Solubility | ||||
μg/cm2 | ||||
CTE | 8° × 10−6/° C.) | Not | ||
(25°-500° C.) | Measured | |||
TABLE 3 |
Example 2 powder with the addition of pigments. |
Glass | |||||||
powder | |||||||
of | |||||||
example | Yellow | Pink | Jet Black | CIE L*a*b* | |||
2 | 41720 | D320 | K-60 | Light Source: | |||
Wt % | Wt % | Wt % | Wt % | D65-10° | |||
99.2687 | 0.7313 | L* | 53.31 | ||||
a* | −2.47 | ||||||
b* | 21.33 | ||||||
C* | 21.47 | ||||||
h* | 96.62 | ||||||
99.6693 | 0.3307 | L* | 55.461 | ||||
a* | 2.10 | ||||||
b* | 0.22 | ||||||
C* | 2.11 | ||||||
h* | 6.06 | ||||||
99.995 | 0.005 | L* | 54.67 | ||||
a* | −0.31 | ||||||
b* | 0.08 | ||||||
C* | 0.32 | ||||||
h* | 164.84 | ||||||
98.6 | 1.4 | ||||||
99.3 | 0.7 | ||||||
99.99 | 0.01 | ||||||
98.933 | 0.7313 | 0.3307 | 0.005 | ||||
98.59 | 0.7 | 0.7 | 0.01 | ||||
Claims (17)
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US09/527,196 US6375729B1 (en) | 1999-03-19 | 2000-03-17 | Machinable glass-ceramics |
US10/066,933 US6645285B2 (en) | 1999-03-19 | 2002-02-04 | Machinable glass-ceramics |
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US12550699P | 1999-03-19 | 1999-03-19 | |
US09/527,196 US6375729B1 (en) | 1999-03-19 | 2000-03-17 | Machinable glass-ceramics |
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US6645285B2 (en) * | 1999-03-19 | 2003-11-11 | Pentron Corporation | Machinable glass-ceramics |
US20070243503A1 (en) * | 2006-04-03 | 2007-10-18 | Jean Gagnon | Method and system for making dental restorations |
US20090221413A1 (en) * | 2004-02-27 | 2009-09-03 | Heraeus Holding Gmbh | Strenghtened, pressable ceramic compositions for dental purposes |
US20090318277A1 (en) * | 2008-06-23 | 2009-12-24 | George Halsey Beall | High strength machinable glass-ceramics |
US20110014589A1 (en) * | 2008-03-19 | 2011-01-20 | Holger Hauptmann | Method for making a dental blank, a press and a system for making dental blanks |
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US10022206B2 (en) | 2004-09-30 | 2018-07-17 | Nobel Biocare Services Ag | Method and system for coloring or tinting a prosthesis, and such a prosthesis |
US10556819B2 (en) | 2017-03-08 | 2020-02-11 | Hass Co., Ltd | Method for preparing glass-ceramics, capable of adjusting machinability or translucency through change in temperature of heat treatment |
WO2020205237A1 (en) | 2019-04-02 | 2020-10-08 | Corning Incorporated | Chemically strengthenable machinable glass-ceramics |
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DE102009008951B4 (en) * | 2009-02-13 | 2011-01-20 | Schott Ag | X-ray opaque barium-free glass and its use |
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